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Refining method of drug intermediate 3, 5-dihydroxybenzyl alcohol

The technology of a dihydroxybenzyl alcohol and a purification method is applied in the field of intermediates of synthetic drugs and the purification field thereof, which can solve the problems of influence of subsequent steps, difficulty in reaching 90% purity, influence on product appearance, etc. Effect

Pending Publication Date: 2022-07-22
南京制药厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The synthesis and separation process of this intermediate is more complicated, and it is difficult to separate and obtain an intermediate product with higher purity. Usually, its purity is difficult to reach 90%, because its crude product contains a large amount of boric acid and borate. It will affect the subsequent process of drugs such as leucectin, especially the color of synthetic leucectin A, which may easily cause the color of leucectin and other drugs to be slightly brown, red and other variegated colors, which will affect the appearance of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: The following sequence is adopted to carry out the purification of the pharmaceutical intermediate 3,5-dihydroxybenzyl alcohol:

[0021] 1) Weigh 100g of crude 3,5-dihydroxybenzyl alcohol and grind it in a mortar, add it to a 2000mL four-neck round bottom flask, add 2g of activated carbon, and add 700g of tetrahydrofuran.

[0022] 2) Start stirring, and slowly heat up to reflux, and maintain the reflux state for 2 hours.

[0023] 3) Filter while hot.

[0024] 4) The filtrate was evaporated under reduced pressure and the solvent was evaporated.

[0025] 5) Add 70g of water, stir, and heat up to 90°C. After the solid is completely dissolved, add solid sodium bicarbonate to adjust the pH of the solution to 7-8.

[0026] 6) Pour the material into a beaker while it is still hot, cool it naturally at room temperature for crystallization, then put the beaker containing the material into an ice-water bath for cooling, stir, cool down to 5°C, and keep for 2 hours...

Embodiment 2

[0030] 1) Pulverize the 3,5-dihydroxybenzyl alcohol intermediate with lower purity with a granulator, accurately weigh 10㎏, add it to a 200L dissolving kettle, first add 60㎏ isopropyl ether to dissolve it, and then add 200g activated carbon.

[0031] 2) Start stirring, and slowly heat up to reflux, and maintain the reflux state for not less than 2 hours.

[0032] 3) Filter while hot, the filtration method used is nitrogen pressure filtration.

[0033] 4) The filtrate is put into another clean kettle, and the filtrate is first distilled at atmospheric pressure, and then switched to vacuum distillation. At the same time, it is heated by circulating hot water to evaporate the solvent.

[0034] 5) Add 7kg of water, stir, and heat up to 90°C. After the solid is completely dissolved, add sodium carbonate solid to adjust the pH value of the solution. The pH value control range: 7-9.

[0035] 6) Put the material into a stainless steel bucket while it is still hot, cool and crystalliz...

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Abstract

The invention discloses a refining method of a drug intermediate 3, 5-dihydroxybenzyl alcohol, which comprises the following steps: crushing a crude product of 3, 5-dihydroxybenzyl alcohol, adding an ether solvent, adding active carbon with a mass ratio of 0.001-0.1, filtering while hot, and distilling filtrate to evaporate the solvent; and then adding water and alkali liquor for dissolving, crystallizing and drying to obtain a refined product of 3, 5-dihydroxybenzyl alcohol. According to the method, decolorization is prior to impurity removal, so that an operator can conveniently monitor the subsequent process, the addition of alkali liquor for dissolution is beneficial to acceleration of the first crystallization speed, and the subsequent recrystallization process greatly improves the purity.

Description

technical field [0001] The present invention relates to an intermediate for synthesizing medicine and its refining technology. Background technique [0002] Leupillin A (3-acetyl-5-hydroxymethyl-7-hydroxy-coumarin) is one of the active ingredients isolated from Pseudomonas pseudocylindrome, and it has been artificially synthesized. Pharmacological studies have shown that it has the effect of promoting bile secretion, has obvious antispasmodic effect on the biliary sphincter, and has the effect of promoting bile secretion and relaxing and antispasmodic effect on the terminal biliary sphincter. Anti-inflammatory, analgesic, antipyretic and other effects, small dose, high safety, is a good drug for patients with acute biliary tract infection, in addition to promoting immune function and enhancing phagocytic phagocytosis. It is clinically used to treat acute and chronic biliary tract infection, viral hepatitis, chronic gastritis, etc., with good curative effect. [0003] The k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/70C07C37/82C07C37/84C07C39/11
CPCC07C37/70C07C37/82C07C37/84C07C37/685C07C39/11
Inventor 陈保才钱肖波王骏
Owner 南京制药厂有限公司
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